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IS 326-11 (1986): Methods of test for natural and synthetic

perfumery materials (Part 11) Determination of carbonyl
value and content of carbonyl compounds [PCD 18: Natural
and Synthetic Fragrance Materials]

“!ान $ एक न' भारत का +नम-ण”

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है”
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“Knowledge is such a treasure which cannot be stolen”
 IS : 326 ( Part 11 ) - 1986
( Reaffirmed 2000 )
Indian Standard
METHODS OF
TEST FOR NATURAL AND SYNTHETIC
PERFUMERY MATERIALS
PART 11 DETERMINATION OF CARBONYL VALUE AND
CONTENT OF CARBONYL COMPOUNDS

( Second Revision )

LJDC 665.572/574:543.854.6

@ Copyright 1987

BUREAU OF INDIAN STANDARDS

MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
*
NEW DELHI 110002

Ct3 July1987
 IS : 326 ( Part 11 ) - 1986

Indian Standard
METHODS OF
TEST FOR NATURAL AND SYNTHETIC
PERFUMERY MATERIALS
PART 11 DETERMINATION OF CARBONYL VALUE AND
CONTENT OF CARBONYL COMPOUNDS

( Second Revision )
Natural and Synthetic Perfumer+ Materials Sectional Committee,
PCDC 18
Chairman Representing
SRRI SHIAN BEHARI LAL Gupta 8s Co ( P ) Ltd, Delhi
Membrrr
SHRI SUDHIR JAIN ( Altmatr to
Shri Shiam Behari La1 )
DR C. K. ATAL RegiFa$; Research Laboratory ( CSIR ), Jammu

DR K. L. DAAR ( Altcrnats )
PROF S.C. BHATTACEARYYA Bose Institute, Calcutta
CHIEF CHEMIST Central Revenues Control Laboratory, New Delhi
DEPUTY CHIEF CEFZ~IST ( AItcrnutc )
SHRI A. K. DAS Directorate General of Technical Development,
New Delhi
SHRI S. K. LUTHRA ( Al&mate )
SERI B. L. GOPALAKRISHNA Karnataka Soaps and Detergents Ltd ( Soap and
Detergent Division ), Bangalore
DR K. B. PATIL ( Aftcrnata )
DR S. S. GOTHOS~AR Indian Pharmacopoeia Committee ( Ministry of
Health & Family Welfare ), New Delhi
SRRI A.K. SHRIVASTAVA (Alternate)
DR RAJENDRA GUPTA Natige;LIBureau of Plant Genetic Resourcea, Now

DR M. L. MAHESHWARI ( Alternate )
DR AKETAR HUSAIN Central Instituteof Medicinal and Aromatic Plants
( CSIR ), Lucknow
DR S. K. JAIN Botanical Survey of India, Calcutta
SRRI V. MUDQAL ( AIternata )
SHPI J. C. KATHRANI Perfumet and Flavours Association of India, Bombay
SHUI AVINASH K. MARATHE ( Alternate )
DR S. U. KULKARNI Hindustan Lever Ltd, Bombay
DR P. CHAKRABORTY (Alternate)
( Continuedon paac 2 )

@ CoHght 1987
BUREAU OF INDIAN STANDARDS
This publtcation is protected under the Indian Copyright Act ( XIV of 19571 and
reproduction in whole or in part by any means except with written permission of the
publisher shall be deemed to be an infringement of copyright under the said Act.
IS : 326 ( Part 11 ) - 1986

( Continuedfrom page 1 )

Members Reprcsentvzg
SHRI G. K. LUTHRIA Mysore Sugandhi Dhoop Factory Ltd, Bomhay
SHHI P. R. MALHANI Development Commissioner (Small Scale Industries),
New Delhi
DR S. K. KAPOOR ( Alternofe )
PROF H. H. MATHUR Indian Institute of Technology, Bombay
PROF G. K. TRIVEDI ( Alternate )
DB R. K. MATH~~R Regional Research Laboratory ( CSIR ), Jorhat
Dn B. K. SAIGIA ( Alternate )
S~nr C. K. MEHROTXA Exnort Insoection Council of India, Calcutta
SHRI S. S. CHOPRA ( Alternafe) ’ ’
DRS.K.MUKHERJEE Indian Agricultural Research Institute, New Delhi
DR N. K. ROY ( Alfernafc )
SHRT T. S. NARAYANASWAMY Swastik Households Industrial Products Ltd. Bombay
DR SHRIDHAR GOPAL PATNEKAR Industrial Perfumes Ltd, Bombay
DR ASHOK DIGAMBER WAGE ( Alternate )
SHRI B. K. PATNEY Richardson Hindustan Ltd, Bombay
SHRI G. S. RANADE ( Ahnate j
DR J. S. PRUTHI Byford Ltd, New Delhi
SHRI P. B. RAO Tata Oil Mills Co Ltd, Bombay
SHRI V. VAIDYANATHAN ( Alternate )
SRKI S. S. REVADI Karnataka Soaps and Detergents Ltd ( Sandalwood
Oil Division ), Mysore
SHRI B. L. GOPALAKRISHNA ( Alternole )
DR S. C. SETHI National Chemical Laboratory ( CSIR ), Pune
DR A. S. RAO ( Alternate ‘I
SRRI N. B. SHANKARACHARYA Central Food Technological Research Institute
( CSIR ), Mysore _
DR K. N. GUR~DUTT ( Alternate )
SHRI S. A. MOHAMBUD SHAREE~ Maschmeijer Aromatics ( India ) Ltd, Madras
SHRI M. I?. SRIVA Forest Research Institute and Colleges, Dehra Dun
SHRI G. S. SHUKLA Directorate of Marketing & Inspection, Faridabad
SHRI R. J. VERMA (Alternate )
DR A. P. SIN~H Camphor & Allied Products Ltd, Bareilly
SHRI S. N. MEHRA ( Alternate )
SHRI I. SUNDARESH Basic Chemicals, Pharmaceuticals and Cosmetic
Export Promotion Council, Bombay
SHRI Y. G. VAIDYA Naarden ( India ) Ltd, Bombay
SHRI S. B. SULE ( Alfernnte )
SHRI R. V. VAZE S. H. Kelkars Co Ltd, Bombay
SHRI M. S. SAXENA, Director General, BIS ( Ex-oficio Member)
Director ( P St C )

Secrcfary
DR ( SMT ) VIJAY MALIE
Assistant Director ( P & C ), BIS

( Contimed on pug.39 )

2
 IS : 326 ( Part 11 ) - 1986

Indian Standard
METHODS OF
TEST FOR NATURAL AND SYNTHETIC
PERFUMERY MATERIALS
PART 11 DETERMINATION OF CARBONYL VALUE AND
CONTENT OF CARBONYL COMPOUNDS

( Second Revision )

0. FOREWORD
0.1 This Indian Standard ( Second Revision ) was adopted by the
Indian Standards Institution on 15 October 1986, after the draft
finalized by the Natural and Synthetic Perfumery Materials Sectional
Committee had been approved by the Petroleum, Coal and Related
Products Division Council.

0.2 This standard was first published in 1952 entitled ‘Methods of test
for essential oils’ and subsequently revised in 1968 as ‘Methods of samp-
ling and test for natural and synthetic perfumery materials’. Taking
cognizance of the need to incorporate instrumental methods of analysis
now in vogue and to facilitate inclusion of additional test methods or
changes in the existing test methods and also to align these test methods
with the corresponding IS0 Standards, the Committee decided to revise
and split t!re standard and publish individual test methods as separate
parts of the original standard.
0.2.1 The test method as given in this part supersedes the test method
as given under 13 of IS : 326-1968*. An amendment in this respect is
being issued separately to the relevant clause of IS : 326-1968*.
0.3 This standard is essentially based on:

a) IS0 1271-1983 Essential oils - Determination of carbonyl value-

Free hydroxylamine method; and
b) IS0 1279- 1973 Essential oils - Determination of carbonyl com-
pounds content - Hydroxylammonium chloride method, publi-
shed by International Organization for Standardization.

*Methods of sampling and test for natural and synthetic perfumery materials (first
re&ion ) .
3
IS : 326 ( Part 11 ) - 1986

0.4 In reporting the result of a test or analysis, made in accordance

with this standard, if the final value, observed or calculated, is to be
rounded off, it shall be done in accordance with IS : 2-1960:

1. SCOPE

1.1 This standard prescribes two methods, namely, hydroxylammonium

chloride and free hydroxylamine methods for the determination of
carbonyl value of a perfumery material by the use of oximation.

2. TERMINOLOGY

2.1 For the purpose of this standard the definitions given in IS : 6597-
1972t shall apply.

2.2 Carbonyl Value - The carbonyl value of a perfumery material

is the mass of potassium hydroxide in mg that is an equivalent to the
mass of hydroxylamine required to oximate the carbonyl compounds
present in 1 g of the oil.

3. DETERMINATION OF CARBONYL VALUE

3.0 General - Two methods, namely, hydroxylammonium chloride

method and free hydroxylamine method are available for determining
the carbonyl value of a perfumery material. Any one of these may be
adopted for the determination of carbonyl value of a perfumery
material, as specified in the individual standard or as may be agreed to
between the purchaser and the supplier. The procedure for the two
methods have been prescribed under 3.1 and 3.2 respectively.
NOTE - It may be pointed out that each of the general methods for determination
as carbonyl value has its place in the analysis of natural and synthetic perfumery
materials. Large difference may be indicative of adulteration with water soluble
constituents or additions of catbonyl compounds of low molecular weight. From a
consideration of the limitations of each method, it should be obvious that it is of
utmost importance always to record the method used when reporting an analytical
result.

3.1 Hydroxylammoniam Chloride Method - Method A

3.1.0 Outline of Method - The carbonyl compounds to be determined

are converted into oximes by reaction with hydroxylammonium chloride.
The hydrochloric acid liberated during the reaction is determined by
an ethanolic potassium hydroxide solution.

*Rules for rounding off numerical values ( revised ).

iGlossary of terms relating to natural and synthetic perfumery materials.

4
 IS : 326 ( Part 11 ) - 1986

3.1.1 Apparatus
3.1.1.1 Conicalflask - 200-ml capacity, with ground-glass stopper.

3.1.1.2 Graduated cylinder - 25-ml capacity ( see IS : 878-1975* ),

3.1.1.3 Burette -- of 25-ml ( see IS : 1997-19677 ).

3.1.2 Reagents

3.1.2.1 Potassium hydroxide - Approximately 0’5 N solution in

95 percent ( U/V) ethanol, standardized immediately before use against
0.5 N hydrochloric acid, using bromophenol blue as indicator and
running the alkali into the acid.

3.1.2.2 Bromophenol blue indicator solution - Dissolve, while warming,

O-2 g of bromophenol blue in 3 ml of ethanolic potassium hydroxide,
0’1 N and 10 ml of ethanol 95 percent ( V/U). After cooling to room
temperature make up to 100 ml with ethanol of the same strength.

3.1.2.3 IYydroxylammonium chloride, ethanolic sol&ion - Dissolve 50 g

of hydroxylammonium chloride in approximately 100 ml of water, and
about 800 ml of 95 percent ( zl/a) ethanol, then IO ml of the ethanolic
bromophenol bIue solution ( 3.1.2.2 ) and dilute to 1 000 ml with 93 per-
cent ( ~J;ID ) ethanol. Add *the ethanolic potassium hydroxicle solution
( 3.1.2.1 ) until the solurion is green, if the liquid is observed in a thin
layer, or until red, if the iayer is thick.

This soiution is suitable for use if a lemon-yellow colour is obtained

when 0.05 ml of the hydrochloric acid is added to 20 ml of the solution,
and a red colour is obtained when 0.05 ml of the potassium hydroxide
solution ( 3.1.2.‘1 ) is added to another 20 ml of the solution.

The solution is stable for 1 week.

3.1.3 Procedure - Weigh, tn the nearest 1 mg, into rhe conical flask
the amount of perfumery material specified In the individual standard.
Add from the graduated cylinder 25 ml of hydroxylammonium chloride
solution and set aside for the time specified in individual standard. If
additional heating is necessary, this will be specified in individual
standard.

After the time prescribed, and if necessary after cooling to room

temperature, titrate the contents of the f.ask with the ethanolic potassium
hydroxide solution, taking care to avoid ,going beyond the greenish-
yellow colour of the indicator, continue the tttration with the potassium
hydroxide solution until a bluish green colour persisting for 5 minutes is
obtained.

*Specification for graduated measuring cylinder.

tSpecification for burettes ( jrst revision ).

5
IS : 326 ( Part 11 ) - 1986

N’cvr~- In the case of perfumery material like oil of vetiver where the acid
value of the oil is high, prior neutralization of the free acids shall be carried out by
taking the required amount of oil ( 0.3 g is normally taken ), accurately weighed
and dissolving in 20 ml of neutral alcohol and neutralizing against 0’5 N alcoh&ic
potassium h) droxide solution.

3.1.4 Calculation - The carbonyl value and content of carbonyl

compounds are calculated as follows:

56’1 x V x N
3.1.4.1 Carbony: value =
m

where

V = volume in ml of ethanolic potassium hydroxide solution

used in the determination;
A’ = the normalitv of 1
the ethanolic potassium hydroxide
solution used; and
m = mass in g of the sample.

3.1.4.2 Content of carbonyl compounds ( as aldehyde or ketone ),

percent by mass

MXVXJV
=
10 m

where
M= molecular mass of the carbonyl compounds in which the
results are to be expressed,
‘V = volume in ml of ethanolic potassium hydroxide solution
used in the determination,
.N = the normality of the ethanolic potassium hydroxide
solution used, and
m = mass in g of the sample.

Express results to the first decimal place.

3.2 Free Hydroxylamine Method - Method B

3.2.0 Outline of the Method - The carbonyl compounds are converted

into oxime by reaction with hydroxylamine freed through the action of
a solution of potassium hydroxide on the hydroxylammonium chloride.
The hydroxylamine remaining after the reaction is determined by
titration with standard hydrochloric acid.
NOTE - This method is suitable for perfumery material containing aldehydes
including citronella1 and certain ketones. in the absence of certain amount of ester
of other alkali sensitive constituents. The method to be used shall be stated in the
specification for the oil.

6
t

1s : 326 ( Part 11 ) - 1986

3.2.1 Apparatus
3.2.1.1 Alkali-resistant glass frask - of capacity 100 to 200 ml, to
which can be fitted by means of a ground-glass joint, a glass tube at
least 1 m long and about 1 cm internal diameter, serving as a reflux
condenser, where required or a glass stopper.
3.2.1.2 Pipette - 20-ml capacity.
3.2.1.3 ConicalJIask - 200-ml capacity, with ground-glass stopper.
3.2.1.4 Burette - lo-ml capacity, graduated in 0’1 ml.
3.2.2 Reagents

3.2.2.1 Hydrochloric acid - 0.5 N.

3.2.2.2 Hydroxylammonium chloride solution - see 3.1.2.3.

3.2.2.3 Bromophenol blue ethanolic solution - see 3.1.2.2.

3.2.2.4 Potassium hydroxide solution - see 3.1.2.1.

3.2.3 Procedure

3.2.3.1 Weigh into a flask to the nearest 1 mg, a mass m of the

perfumery material as prescribed in individual standard. Introduce by
means of a pipette, 20 ml of hydroxylammonium chloride into a conical
flask. Add 10 ml of potassium hydroxide solution measured from a
burette. Mix it well.
Pour the liquid into the flask containing the perfumery material
and reserve the conical flask without washing. In case of aldehydes,
allow to stand for 15 minutes at room temperature while for ketones,
reflux gently for one hour using a water condenser or an air condenser
at least 75 cm long. Cool to room temperature ( see Note below ). Where
the individual standard specifies, add bromophenol blue indicator ( as for
dark coloured perfumery materials ).
NOTE - Some aldehydes or ketones have been found to require longer standing
or heating. In such case the change will be noted under the individual standard.

Neutralize with hydrochloric acid contained in the burette till a

greenish-yellow colour is observed. Transfer the liquid to the conical
flask used to mix the reagent and the alcoholic potassium hydroxide
solution, and pour about half back again into the flask. Continue the
neutralization in one of the flask only till the greenish-yellow colour of
the indicator changes to lemon-yellow. The colour obtained in both
flasks, shall not alter further when two drops of 0’5 N hydrochloric acid
are added.
Alternatively this titration may be carried out by a potentiometric
method to pH 3.3.
7
IS:326(Partlf)-1986

3.2.3.2 Blank determination - Simultaneously with the determination

prescribed in 3.2.3, carry out a blank test with the same reagents and
following the same procedure but omitting the perfumery material.
3.2.4 Calculation

3.2.4.1 The carbonyl value is calculated as follows:

56.1 x ( V, - V2 ) N
Carbonyl value ==
m

where
VI = volume in ml of standard hydrochloric acid used in the
blank titration,
Vs == volume in ml of standard hydrochloric acid used in the
determination,
.h’ = the normality of the hydrochloric acid used for titration,
and
tn = mass in g of the sample.
3.2.4.2 The content of carbonyl compounds expressed in terms of
designated aldehydes and ketones is calculated as follows:
Content of carbonyl
compounds ( as aldehydes = M ( VI - v2 1
20 m
and ketones ), percent
by mass
wherl
M- molecular mass of the aldehyde or ketones specified in
the individual standard for the particu!ar perfumery
material,
Vl - volume in ml of standard hydrochloric acid used in the
blank titration,
v2 - volume in ml of standard hydrochloric acid used in the
determination, and
m= mass in g of the sample taken.
E-r- the results to the first place of decimal.
NOTE - In this, it is assumed that the alohols are monohydric and acids
monobasic.

8
 IS : 326 ( Part 11 ) - 1986

( Continued j?om page 2 )

Composition of Methods of Test Subcommittee, PCDC 18 : I

Conz~ener Repesenting
SIIRI S. N. h’fWfItA Canlphor & Allied Products Ltd, Bareilly
Aiembers
1)~: K. 0. AlrllArInnr Central Food Technological Research Institute
( CSIR ). Mysore
DIL J. N. HAIIUAII Regional Research Laboratory ( CSIR ), Jorhat
II.. .,
SJlltI B. ~Kll3l~AIIMANrAX ( .'llle~?Zale
I
()FBICR INCli,\lloE Forebt Research Institute & Colleges, Dehra Dun
Dn 1%.B. Grr.k~oil: National Chemical I,ahoratory ( CSIR ), Pune
Srrlrr Sunnm JAIN Gupta & Co (I’) Ltd Delhi
I’I<OF‘I?. R. K,\STUI<I Indian Institute of Science, Bangalore
PIIOF G. S. R. SUBRARAO ( Alternnte)
SHILI G. D. KELI<>\R Gupta & Co (P) Ltd, Delhi
Da S. U. KULRAXNI Hindustan Lever Ltd, Bombay
Dn S. N. K. CHOUDIXO~I ( Alternate )
Dn M. L. MAI~ES~W.\I<I National Bureau of Plant Genetic Resources,
New Delhi
I’no~ H. H. MATHTJR Indian Institute of Technology, Bombay
DR SI~II)~IAI~ Gopa~ PATNIXAR Industrial Perfumes Ltd, Bombay
DR ASHOICDI~AMBER Wao~ ( Alternate )
SHRI P. B. RAO Tata Oil Mills Co Ltd, Bombay
SHRI V. VAIDYANATHAN I Alternate 1
SIXRI ATUL SINEA ’ __ Directorate-of Marketing and Inspection, Nagpur
SREI T. V. MATHEW ( Alternate )
SHI~I SANTOSHYE:LCORE Analytical Testing Services Pvt Ltd, New Delhi
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